CN116288790A - High-strength high-modulus fine denier polyarylester fiber - Google Patents
High-strength high-modulus fine denier polyarylester fiber Download PDFInfo
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- CN116288790A CN116288790A CN202310049819.6A CN202310049819A CN116288790A CN 116288790 A CN116288790 A CN 116288790A CN 202310049819 A CN202310049819 A CN 202310049819A CN 116288790 A CN116288790 A CN 116288790A
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- polyarylate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention discloses a high-strength high-modulus fine denier polyarylate fiber and a preparation method thereof, wherein the monofilament linear density of the high-strength high-modulus fine denier polyarylate fiber is less than 2D, the breaking strength of a bundle wire after heat treatment is more than 27cN/dtex, and the tensile modulus of the bundle wire after heat treatment is more than 800cN/dtex; the preparation method comprises the following steps: (1) drying the high molecular weight polyarylate resin; (2) Feeding the high molecular weight polyarylate resin into a discharge barrel of a double-screw extruder with nitrogen protection, conveying the resin into the double screws, and simultaneously feeding four modified siloxanes; (3) Extruding, drawing and rolling to obtain a fine denier polyarylate fiber primary yarn; (4) And carrying out heat treatment on the primary filaments of the fine denier polyarylate fibers to obtain the high-strength high-modulus fine denier polyarylate fibers. The invention can realize the high-efficiency preparation of the high-strength high-modulus fine denier polyarylester fiber, improves the spinning efficiency and the heat treatment efficiency, saves energy, improves the product diversification, improves the physical properties of the product, and greatly improves the competitiveness of the product.
Description
The present application is a divisional application. Parent application number: 202011022132.6, filing date: 09 month 25 of 2020, invention name: a high-strength high-modulus fine denier polyarylate fiber and a preparation method thereof.
Technical Field
The invention relates to the technical field of organic chemistry, in particular to a high-strength high-modulus fine denier polyarylate fiber.
Background
The polyarylate fiber is a special fiber with excellent comprehensive properties of high strength, high modulus, high temperature resistance, low water absorbability, self-flame retardance, high wear resistance, chemical resistance, radiation resistance, strong dimensional stability and the like, and is widely applied to the application fields of bulletproof, cutting prevention, stab prevention, composite reinforcement, cable ropes and the like. The fine denier of the fiber enables the prepared fabric structure to have specific interface properties, micro-cavity structures can be formed in the fabric, the fabric can be mutually penetrated with other materials, and the like, and the comprehensive performance of the composite material can be improved by matching with high-strength high-modulus performance. The rigid chain structure of the molecular structure of the liquid crystalline polyarylate fiber determines that it cannot obtain finer fiber diameters using a means of hot drawing, and thus, the diameter of the nascent fiber is its final diameter. The preparation of finer liquid crystal polyarylester fibers is always a difficult problem at home and abroad, and the monofilament linear density of the Vectran fibers which are circulated in the market is 5D, and the Vectran fibers are coarser than other special fibers. In order to obtain the liquid crystal polyarylate fiber with smaller fineness, the Japanese colali company adopts an island-in-sea spinning method, but the method has the disadvantages of complex process, high cost and low practicability. Patent CN200880006177, patent CN201810261002, all mentions that polyarylate is fibrillated by extrusion from a spinneret at a temperature above the melting point, and further the physical properties of the fiber are improved by heat treatment, but none mention a method for preparing a high-strength high-modulus fine denier polyarylate fiber.
In the method of spinning fine denier fibers in "islands-in-the-sea" type, there is a problem that the cost is extremely high in industrial production because a special spinning nozzle having a complicated structure, a special process for elution, segmentation, or the like is required at the stage of melt spinning, and the like. It is known that the polyarylate melt is in a liquid crystal state below a clear point above a melting point, the melt basically has no extrusion swelling effect at an outlet of a spinneret orifice, and is quickly solidified about 10cm below a spinneret plate, but when the high molecular weight liquid crystal polyarylate is used for spinning fibers, the viscosity is too large, the shearing or stretching effect is insufficient before the polyarylate enters the spinneret orifice, the viscosity is very large, and only a spinneret plate with larger aperture can be used, so that the high-temperature and high-pressure melt can be smoothly extruded, the requirements on the temperature control precision of equipment and the pressure resistance of the equipment are improved, and meanwhile, the method cannot effectively realize the high-nozzle stretching ratio to ensure that the fibers are spun more finely.
Disclosure of Invention
The invention aims to overcome the technical defects of the background technology and provide a high-strength high-modulus fine denier polyarylate fiber and a preparation method thereof. The invention solves the technical problems of poor fluidity and harsh spinning conditions of the high molecular weight polyarylate resin, can smoothly carry out fine denier spinning on the high molecular weight polyarylate resin, and does not need to bring strict requirements to equipment; the method is simple to operate, can be implemented under the condition of not changing the original polyarylate melt spinning and heat treatment equipment, and has high practical application value; the invention can realize the high-efficiency preparation of the high-strength high-modulus fine denier polyarylester fiber, improves the spinning efficiency and the heat treatment efficiency, saves energy, improves the product diversification, improves the physical properties of the product, and greatly improves the competitiveness of the product.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of high-strength high-modulus fine denier polyarylate fiber comprises the following steps:
(1) Drying raw materials: drying the raw material high molecular weight polyarylate resin to remove moisture; the high molecular weight polyarylate resin has a molecular weight of >30w;
(2) Melt blending: putting the dried high molecular weight polyarylate resin into a discharging barrel of a double-screw extruder with nitrogen protection, and continuously conveying the resin into the double screw at a certain melt spinning temperature; simultaneously, precisely adding a certain proportion of modified siloxane into the double screw rods by using a weightless balance feeding system; the modified siloxane comprises polyhydroxy methyl siloxane, polyphenyl methyl siloxane, hydroxy polyphenyl methyl siloxane and polyhydroxy phenyl siloxane; the input proportion of each modified siloxane is 0.3-10 mol% of the input amount of the high molecular weight polyarylate resin;
(3) Extrusion winding: extruding, drawing and rolling the fiber with high spray head stretching ratio under the double-screw spinning process to obtain a fine denier polyarylate fiber primary yarn;
(4) And (3) heat treatment: and carrying out heat treatment on the primary filaments of the fine denier polyarylate fibers at the optimal heat treatment temperature to obtain the high-strength high-modulus fine denier polyarylate fibers.
Preferably, in the step (1), the polyarylate resin may be a mixed melt polymerization of monomers such as two or more of parahydroxybenzoic acid, hydroquinone, terephthalic acid, isophthalic acid, 6-hydroxy 2-naphthoic acid, biphenyl, resorcinol, naphthalene diphenol.
Preferably, in the step (1), the high molecular weight polyarylate resin has a molecular weight of 30w to 40w; more preferably 35w, the melt viscosity is 60 pa.s and the melting point is 310 ℃.
Preferably, in the step (1), the high molecular weight polyarylate resin is dried in a vacuum drying oven at 150 ℃ to remove moisture.
Preferably, in the step (2), the melt spinning temperature is 250 to 350 ℃.
Preferably, in the step (2), the molar mass ratio of the polyhydroxymethylsiloxane, the polyphenylmethylsiloxane, the hydroxypolyphenylmethylsiloxane and the polyhydroxyphenylsiloxane is (0.3-2): (1-10): (0.3-4): (4-6).
Preferably, in the step (3), the temperature at the time of extrusion is 315 to 350 ℃; more preferably 320 to 340 ℃; more preferably 325 to 330 ℃.
Preferably, in the step (3), the screw pressure during extrusion is 4-8 Mpa; more preferably 5 to 7MPa; more preferably 6MPa.
Preferably, in the step (3), the temperature of the assembly during extrusion is 315-350 ℃; more preferably 320 to 340 ℃; more preferably 325 to 330 ℃.
Preferably, in the step (3), the assembly pressure during extrusion is 3-7 Mpa; more preferably 3.5 to 6MPa; more preferably 4 to 5MPa.
Preferably, in the step (3), the diameter of the spinneret plate during extrusion is 0.1-0.5 mm; more preferably 0.15 to 0.3mm; further preferably 0.16mm.
Preferably, in the step (3), the number of spinneret holes during extrusion is 1 to 1000f; more preferably 10 to 100f; further preferably 20f.
Preferably, in the step (3), V at the time of the extrusion 0 10-40 m/min; more preferably 15 to 30m/min; more preferably 20 to 25m/min.
Preferably, in the step (3), V at the time of the extrusion f 200-5000 m/min; more preferably 1000 to 4000m/min; more preferably 1800 to 3800m/min.
Preferably, in the step (3), the stretching ratio of the nozzle during the stretching is 20-300; more preferably 50 to 200; more preferably 80 to 160.
Preferably, in the step (4), the temperature at the time of the heat treatment is 240 to 300 ℃; more preferably 250 to 280 ℃; further preferably 260 ℃.
Preferably, in the step (4), the time during the heat treatment is 5 to 50 hours; more preferably 8 to 30 hours; further preferably 10 hours.
The high-strength high-modulus fine denier polyarylate fiber is prepared by adopting the preparation method of the high-strength high-modulus fine denier polyarylate fiber.
Preferably, the high-strength high-modulus fine denier polyarylate fiber has a filament linear density of < 2D, a bundle fiber breaking strength of >27cN/dtex after heat treatment, and a bundle fiber tensile modulus of >800cN/dtex after heat treatment.
The preparation method of the high-strength high-modulus fine denier polyarylate fiber can also be used for preparing the high-strength high-modulus special-shaped hollow polyarylate fiber.
The basic principle of the invention is as follows:
the present invention has been made in an intensive study on a finely denier polyarylate fiber capable of stably spinning a high molecular weight using conventional equipment and processes, and a process for preparing a high-strength, high-modulus finely denier polyarylate fiber by heat treatment, and as a result, has found the present invention.
The invention provides a high-strength high-modulus fine denier polyarylate fiber and a preparation method thereof, which improve the fluidity of polyarylate, and particularly aim at improving the liquid crystal polyarylate spinning process with higher molecular weight to prepare the high-strength high-modulus fine denier liquid crystal polyarylate fiber. Compared with the liquid crystal polyarylester with low molecular weight, the nascent fiber prepared by the liquid crystal polyarylester with high molecular weight has higher strength, and can reach higher level only by heat treatment of the mechanical property of the fiber for a short time, thereby greatly improving the production efficiency and the productivity. However, for the liquid crystal polyarylester spinning with high relative molecular mass, the melt viscosity of the system is higher, the requirements on temperature control precision and equipment pressure resistance are higher, the spinning difficulty is increased, and the conventional process cannot be used for preparing the fine denier fiber with high spray head stretching ratio, so that the melt viscosity is required to be reduced by a special method. The invention adopts a double-screw extruder for spinning, improves the spinning fluidity of the liquid crystal polyarylate with higher molecular weight by adding modified siloxane, and prepares the high-strength high-modulus fine denier liquid crystal polyarylate fiber.
Specifically, in the process of double-screw melt spinning, four modified siloxanes (polyhydroxy methyl siloxane, polyphenyl methyl siloxane, hydroxy polyphenyl methyl siloxane and polyhydroxy phenyl siloxane) with a certain proportion are added and introduced in the high molecular weight polyarylate resin blanking stage so as to achieve interface lubrication, reduce the surface adhesion of the resin, improve the fluidity of the high molecular weight polyarylate resin in the screw and improve the trafficability of the polyarylate resin in a component and a spinneret plate, thereby reducing the requirement on too severe equipment in the high molecular weight polyarylate melt spinning, preparing the fine denier polyarylate fiber under a higher spray head stretching ratio, preparing the high-strength high-modulus fine denier polyarylate fiber through short-time heat treatment, and realizing the improvement of fiber quality, production efficiency and cost reduction.
Wherein, hydroxyl (-OH) on the molecular chain of the modified siloxane containing hydroxyl is subjected to polycondensation reaction with carboxyl (-COOH) on the tail end of the polyarylate macromolecule in the process of double-screw melt extrusion, and the formed chemical bond enables the siloxane to be anchored on the polyarylate macromolecule chain and not easy to escape; the chain flexibility of the modified siloxane containing methyl is high, so that the internal lubricity of an interface can be improved, the surface adhesion of the resin is reduced, and the flowability of the resin is improved; the hydroxyl-containing modified siloxane and the methyl-containing modified siloxane can play a synergistic interaction role, so that the flowability of the resin in a screw, a component and a spinneret plate is improved to a greater extent.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention solves the technical problems of poor fluidity and harsh spinning conditions of the high molecular weight polyarylate resin, can smoothly carry out fine denier spinning on the high molecular weight polyarylate resin, and does not need to bring strict requirements to equipment;
(2) The method is simple to operate, can be implemented under the condition of not changing the original polyarylate melt spinning and heat treatment equipment, and has high practical application value;
(3) The invention can realize the high-efficiency preparation of the high-strength high-modulus fine denier polyarylester fiber, improves the spinning efficiency and the heat treatment efficiency, saves energy, improves the product diversification, improves the physical properties of the product, and greatly improves the competitiveness of the product.
Detailed Description
For a better understanding of the present invention, reference will be made to the following description of specific examples. It is to be understood that these examples are provided only for further illustration of the present invention and are not intended to limit the scope of the present invention. It should be further understood that after reading the description of the present invention, those skilled in the art make some insubstantial changes or modifications to the present invention, which still fall within the scope of the present invention.
In examples 1 to 7 and comparative examples 1 to 6, the polymer A was a high molecular weight polyarylate resin having a molecular weight of 35w, a melt viscosity of 60 pa-s, and a melting point of 310 ℃; the polymer B is a low molecular weight polyarylate resin, the molecular weight of the polymer B is 25w, the melt viscosity of the polymer B is 40 pa-s, and the melting point of the polymer B is 280 ℃.
In examples 1 to 7 and comparative examples 1 to 6, the number of holes of the spinneret plate used for spinning was 20f.
A preparation method of high-strength high-modulus fine denier polyarylate fiber comprises the following steps:
(1) Drying raw materials: drying the raw material high molecular weight polyarylate resin to remove moisture;
(2) Melt blending: putting the dried high molecular weight polyarylate resin into a discharging barrel of a double-screw extruder with nitrogen protection, and continuously conveying the resin into the double screw at a certain melt spinning temperature; simultaneously, precisely adding a certain proportion of modified siloxane into the double screw rods by using a weightless balance feeding system; the modified siloxane comprises polyhydroxy methyl siloxane, polyphenyl methyl siloxane, hydroxy polyphenyl methyl siloxane and polyhydroxy phenyl siloxane; the input proportion of each modified siloxane is 0.3-10 mol% of the input amount of the high molecular weight polyarylate resin;
(3) Extrusion winding: extruding, drawing and rolling the fiber with high spray head stretching ratio under the double-screw spinning process to obtain a fine denier polyarylate fiber primary yarn;
(4) And (3) heat treatment: and carrying out heat treatment on the primary filaments of the fine denier polyarylate fibers at the optimal heat treatment temperature to obtain the high-strength high-modulus fine denier polyarylate fibers.
Comparative example 1
A method for preparing a polyarylate fiber, comprising the steps of:
(1) Drying the polymer A in a vacuum drying oven at 150 ℃ to remove water;
(2) Melting Polymer A with a twin-screw extruderSpinning (without addition of modified siloxane) in which the extrusion temperature was 350℃and the screw pressure was 6MPa, the spinneret temperature was 350℃and the assembly pressure was 6MPa, the spinneret aperture was 0.3mm and the free-falling speed V 0 20m/min, maximum spinnability V f 600m/min, a spray head stretching ratio of 30, and a primary fiber with a primary tow strength of 8.54cN/dtex;
(3) And (3) carrying out heat treatment on the nascent fiber at the temperature of 290 ℃ for 15 hours to obtain the polyarylate fiber, wherein the filament linear density is 5D, the strand breaking strength is 24cN/dtex, and the tensile modulus is 730cN/dtex.
Specifically, the technological parameters involved in the preparation process of the polyarylate fibers of examples 1 to 7 and comparative examples 1 to 6 and the mechanical property test results of the prepared polyarylate fibers are shown in table 1:
table 1 results of mechanical property test of the polyarylate fibers prepared by the process parameters involved in the preparation of the polyarylate fibers of examples 1 to 7 and comparative examples 1 to 6
The method for measuring the melting point comprises the following steps: a sample of 10 to 20mg was taken in a DSC apparatus, sealed in an aluminum pan, and then, 50cc/min of nitrogen gas was introduced, and the temperature rise rate of 10℃per minute was measured, and Tm was the peak of the endothermic peak. Depending on the type of polymer, there are cases where no distinct endothermic peak appears in the first measurement. At this time, the Tm can be measured by heating at a heating rate of 40℃per minute for about 4 minutes or so at a temperature higher than the temperature at which the insignificant endothermic peak appears and then cooling at 50℃per minute to 25℃and then measuring the Tm at the same heating rate of 10℃per minute.
The method for measuring the melt viscosity comprises the following steps: the temperature of the polyarylate sample was raised to Tm+20℃by a capillary rheometer, and when the sample passed through a nozzle of 0.5mm, a shear rate of 1000sec-1 was applied, and the viscosity at this time was measured as melt viscosity MV.
From the experimental data of examples 1 to 7 and comparative examples 1 to 6, the present invention has been studied to find that:
(1) The addition of the modified siloxane can improve the fluidity of the low-molecular weight and high-molecular weight polyarylate resin and reduce the melt viscosity;
(2) The improvement of the fluidity of the polyarylate resin is inferior to that of the mixed addition of the two types by only adding the siloxane modified by hydroxyl or not modified by hydroxyl, and the strength modulus of the prepared fiber is relatively lower than that of the mixed addition of the two types;
(3) The high molecular weight polyarylate resin can realize the melt viscosity (about 40 pa-s) close to that of the low molecular weight polyarylate resin after four modified siloxanes are added, can reach higher highest spinning speed and obtain primary fibers with higher strength, but can prepare fibers with higher relative strength modulus by shorter heat treatment time;
(4) When the content of the modified siloxane is excessively added, the fluidity of the modified siloxane to the polyarylate resin can be still improved, but the mechanical property of the fiber is not increased and reduced.
The four modified siloxanes are added to realize high-speed fine denier spinning with high molecular weight polyarylester and high spray head stretching ratio, so that the spinning efficiency and the heat treatment efficiency are improved, the energy is saved, the diversity of products is improved, the mechanical properties of the prepared heat treatment fiber are also improved, and the competitiveness of the products is greatly improved.
The above description is not intended to limit the invention, nor is the invention limited to the examples described above. Variations, modifications, additions, or substitutions will occur to those skilled in the art and are therefore within the spirit and scope of the invention.
Claims (3)
1. The high-strength high-modulus fine denier polyarylate fiber is characterized in that the monofilament linear density of the high-strength high-modulus fine denier polyarylate fiber is less than 2D, the breaking strength of the heat-treated bundle filaments is more than 27cN/dtex, and the tensile modulus of the heat-treated bundle filaments is more than 800cN/dtex;
the preparation method of the high-strength high-modulus fine denier polyarylate fiber comprises the following steps:
(1) Drying raw materials: drying the raw material high molecular weight polyarylate resin to remove moisture; the molecular weight of the high molecular weight polyarylate resin is 30 w-40 w;
(2) Melt blending: putting the dried high molecular weight polyarylate resin into a discharging barrel of a double-screw extruder with nitrogen protection, and continuously conveying the resin into the double screw at a certain melt spinning temperature; simultaneously, precisely adding a certain proportion of modified siloxane into the double screw rods by using a weightless balance feeding system; the modified siloxane comprises polyhydroxy methyl siloxane, polyphenyl methyl siloxane, hydroxy polyphenyl methyl siloxane and polyhydroxy phenyl siloxane; the input proportion of each modified siloxane is 0.3-10 mol% of the input amount of the high molecular weight polyarylate resin;
(3) Extrusion winding: extruding, drawing and rolling the fiber with high spray head stretching ratio under the double-screw spinning process to obtain a fine denier polyarylate fiber primary yarn;
(4) And (3) heat treatment: carrying out heat treatment on the primary filaments of the fine denier polyarylate fibers at the optimal heat treatment temperature to obtain high-strength high-modulus fine denier polyarylate fibers;
in the step (2), the melt spinning temperature is 250-350 ℃;
in the step (2), the molar mass ratio of the polyhydroxymethylsiloxane to the polyphenylmethylsiloxane to the hydroxypolyphenylmethylsiloxane is (0.3-2) to (1-10) to (0.3-4) to (4-6);
in the step (3), the temperature during extrusion is 315-350 ℃; the screw pressure during extrusion is 4-8 Mpa; the temperature of the assembly during extrusion is 315-350 ℃; the pressure of the assembly during extrusion is 3-7 Mpa; the aperture of the spinneret plate during extrusion is 0.1-0.5 mm; the number of spinneret holes during extrusion is 1-1000 f; v at the time of extrusion 0 10-40 m/min; v at the time of extrusion f 200-5000 m/min; spray head draw ratio during the drawing20 to 300 percent;
in the step (4), the temperature during the heat treatment is 240-300 ℃; the time for the heat treatment is 5-50 h.
2. The high strength, high modulus, fine denier polyarylate fiber of claim 1, wherein said high molecular weight polyarylate resin in step (1) has a molecular weight of 35w, a melt viscosity of 60 pa-s, and a melting point of 310 ℃.
3. The high strength, high modulus, fine denier polyarylate fiber of claim 1, wherein said high molecular weight polyarylate resin is dried in a vacuum oven at 150 ℃ to remove moisture in step (1).
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| CN202310049819.6A CN116288790A (en) | 2020-09-25 | 2020-09-25 | High-strength high-modulus fine denier polyarylester fiber |
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